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A kind of method for preparing β-aminopropionic acid with high selectivity

A technology of aminopropionic acid and acrylic acid, applied in the field of chemistry, can solve problems such as being unfavorable for large-scale use, low yield and selectivity, and achieve the effects of improved selectivity, improved overall yield and beneficial purification

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lower yield and selectivity are not conducive to the large-scale use of this route

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The acrylic acid and the ammonia water with a concentration of 35wt% are put into the reaction kettle in a molar ratio of acrylic acid:ammonia=1:7, and the additions of cobalt chloride and 4,4'-dicarboxy-2,2'-bipyridine are respectively: 5 mol% and 10 mol% of acrylic acid, after the reaction kettle is sealed, the reaction temperature is controlled at 80° C., the pressure is controlled at 1.0 MPa, and the reaction is held at a constant temperature for 3 hours. After the reaction is completed, the conversion rate of acrylic acid is detected by sampling and detection is greater than 99%. Excess ammonia is absorbed by ammonia absorption pump, and then concentrated under reduced pressure until the reaction liquid is syrupy, and methanol with 7 times the initial weight of acrylic acid is added. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The obtained crystal is β-aminopropionic acid after suction filtration and drying. The obtaine...

Embodiment 2

[0018] The acrylic acid and the ammonia water with a concentration of 35% are put into the reaction kettle in a molar ratio of acrylic acid: ammonia=1:10, and the additions of cobalt chloride and 4,4'-dicarboxy-2,2'-bipyridine are respectively 9 mol% and 15 mol% of acrylic acid, after the reactor is sealed, the reaction temperature is controlled at 130° C., the pressure is controlled at 1.7MPa, and the constant temperature reaction is performed for 0.5h. After the reaction is completed, the conversion rate of acrylic acid is detected by sampling to be greater than 99%, and the excess ammonia is absorbed by an ammonia absorption pump, and then the reaction solution is concentrated under reduced pressure until the reaction liquid is syrupy, and methanol with 8 times the weight of acrylic acid is added. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The obtained crystal is β-aminopropionic acid after suction filtration and drying. The ob...

Embodiment 3

[0020] The acrylic acid and the ammonia water with a concentration of 30% are put into the reaction kettle in a molar ratio of acrylic acid: ammonia=1:10, and the additions of nickel chloride and 5,5'-dicarboxy-2,2'-bipyridine are respectively: 8 mol% and 13 mol% of acrylic acid, after the reaction kettle is sealed, the reaction temperature is controlled at 120 ° C, the pressure is controlled at 1.5 MPa, and the reaction is held at a constant temperature for 1 h. After the reaction was completed, the conversion rate of acrylic acid was detected by sampling to be greater than 99%, and excess ammonia was absorbed by an ammonia absorption pump, and then the reaction solution was concentrated under reduced pressure until the reaction solution was syrupy, and methanol was added with 9 times the weight of acrylic acid. Continue to stir and reflux at this temperature for 1 h, then cool down and crystallize. The obtained crystal is β-aminopropionic acid after suction filtration and dr...

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Abstract

The invention discloses a method for preparing β-aminopropionic acid from acrylic acid. It comprises the following steps: in the kettle type reactor, acrylic acid and ammonia water react in the presence of a catalyst and a ligand, and then the reaction solution is subjected to deamination, concentration and crystallization to prepare β-aminopropionic acid; wherein the catalyst is Transition metal inorganic salt, the ligand is a pyridine ligand. The invention has the advantages of good product selectivity, high yield, convenient purification, mild process conditions and the like. Experiments show that after the catalyst and ligand are introduced, the conversion rate of acrylic acid is greater than 99%, the single-pass product yield of the reaction is greatly increased to 82%, the difficulty of later purification is greatly reduced, and the mother liquor can be recycled, and the cycle yield is greater than 95%.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a preparation method of beta-aminopropionic acid. Background technique [0002] β-aminopropionic acid, as the only β-amino acid in nature, is mainly used as a key intermediate in the synthesis of calcium pantothenate (vitamin B5). In addition, it is also widely used in medicine, food and other fields, and has a good market prospect. At present, the methods for producing β-aminopropionic acid mainly include acrylonitrile amination hydrolysis method, enzymatic method and acrylic acid amination method. Among them, the acrylonitrile method has a long route, and is accompanied by the formation of a large amount of inorganic salts after hydrolysis, making purification more difficult. The enzymatic method mainly uses L-aspartic acid as a raw material, which is catalyzed by L-aspartic acid decarboxylase, and the production cost is relatively high, and it is accompanied by ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/08C07C227/08C07C227/40C07C227/42
CPCC07C227/08C07C227/40C07C227/42C07C229/08
Inventor 李胜勇孔令晓张涛
Owner WANHUA CHEM GRP CO LTD
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